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Reagent preparation method

A technology of reagents and reaction bottles, applied in the field of organic synthesis, can solve the problems of non-reaction and incompleteness, and achieve the effect of short reaction time

Inactive Publication Date: 2014-02-05
NORTHWEST A & F UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problem that nitrogen-chloro-succinimide or trichloroisocyanuric acid is used as a chlorine source in an organic solvent to react incompletely or substantially without reaction, the invention provides a reagent preparation method

Method used

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Embodiment 1

[0019] The embodiment of the present invention only takes the synthesis method of bis(2-ethyl)hexyl chlorophosphate as an example to illustrate, and the details are as follows:

[0020] Concretely, in 50 milliliters of dry two-necked flasks, add 36 millimoles, the N-chlorosuccinimide of 4.807 grams;

[0021] Add a magnetic stirrer, one bottle mouth is connected to the vacuum argon gas pipeline, and the side bottle mouth is installed with a flip-top rubber stopper to replace the atmosphere in the bottle with argon gas;

[0022] Place the device in an ice bath and turn on magnetic stirring. 30 millimoles, 9.193 grams of bis(2-ethyl)hexyl phosphite were continuously added dropwise from the rubber stopper with a syringe;

[0023] After stirring for 2 hours the liquid product was filtered off.

[0024] Preferably, in order to increase the yield, the solid can be washed twice with a small amount of anhydrous hexane, combined with the first filtrate and then concentrated to remove ...

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PUM

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Abstract

The invention discloses a reagent preparation method, and belongs to the field of organic synthesis. The reagent preparation method comprises the following steps: adding a preset amount of N-chlorosuccinimide to a reaction flask; replacing air in the reaction flask with inert gas, and cooling the reaction flask to a preset temperature; dropwise adding phosphorous acid diester to the reaction flask; when ending the reaction, diluting by using a preset amount of anhydrous solvent, and filtering an diluted product; and concentrating the product, thus obtaining diester chlorophosphate. The reagent preparation method has the advantages that no solvent is used in an ester chlorophosphate reaction process, the reaction can be completely carried out, the reaction time is short, and liquid waste is not generated; under normal circumstances, the obtained product has enough high purity and meets the requirements of common organic synthesis, and if the purity is unsatisfactory, the product can be further distilled.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a reagent preparation method. Background technique [0002] Dihydrocarbyl chlorophosphate is an important reagent for the synthesis of organophosphorus compounds, especially phosphoric acid mixed ester compounds. Dihydrocarbyl chlorophosphate is prepared by reacting phosphite with gaseous chlorine sources such as chlorine and phosgene. After the reaction, it is necessary to use dry air and lead carbonate to remove the dissolved gas and acid in the product. Generate solid waste that pollutes the environment. In the prior art, nitrogen-chloro-succinimide or trichloroisocyanuric acid is used as the chlorine source. [0003] In the process of realizing the present invention, the inventor finds that there are at least the following problems in the prior art: [0004] The preparation method of prior art uses acetonitrile or toluene as solvent, produces unnecessary liquid waste; The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/14
Inventor 仲崇民左亚杰
Owner NORTHWEST A & F UNIV
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